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SN/T 5259-2020: (Determination of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in coatings gas chromatography-mass spectrometry)
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| SN/T 5259-2020 | English | 199 |
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(Determination of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in coatings gas chromatography-mass spectrometry)
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SN/T 5259-2020
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Basic data | Standard ID | SN/T 5259-2020 (SN/T5259-2020) | | Description (Translated English) | (Determination of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in coatings gas chromatography-mass spectrometry) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | G51 | | Classification of International Standard | 87-010 | | Word Count Estimation | 9,956 | | Date of Issue | 2020-08-27 | | Date of Implementation | 2021-03-01 | | Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] | | Issuing agency(ies) | General Administration of Customs | SN/T 5259-2020: (Determination of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in coatings gas chromatography-mass spectrometry)
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The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2020-08-27 released
2021-03-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2020.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organization of this standard. Guangzhou Customs of the People's Republic of China.
The main drafters of this standard. Zheng Jianguo, Wang Jing, Zhang Zihao, Liu Yingfeng, Li Quanzhong, Xiao Qian, Zhai Cuiping, Zhou Minghui, Peng Ying,
Li Chunyan, Yu Jianlong, Xiao Dahui
Gas chromatography-mass spectrometry
1 Scope
This standard specifies the content of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in water-based paints and solvent-based paints
The gas chromatography-mass spectrometry detection method.
This standard applies to the content of UV-320, UV-327, UV-328 and UV-350 ultraviolet absorbers in water-based paints and solvent-based paints
The determination.
2 Method summary
The sample is leveled on a clean glass sheet, and after natural air drying, the solvent-based paint is ultrasonically extracted with n-hexane, and the water-based paint is ultrasonically extracted with acetonitrile.
Sound extraction. After the extract is concentrated, it is purified by a solid phase extraction column, filtered by a filter membrane, and measured with a gas chromatography-mass spectrometer. External standard
Method quantitative.
3 Reagents and materials
Unless otherwise stated, all reagents are chromatographically pure.
3.1 Methanol.
3.2 n-hexane.
3.3 Acetonitrile.
3.8 Single standard stock solution of ultraviolet absorber. accurately weigh the appropriate amount of UV-320 standard material (3.4), UV-327 standard material (3.5),
UV-328 standard material (3.6) and UV-350 standard material (3.7), respectively use methanol (3.1) to make a constant volume, and prepare a concentration of 1 000 mg/L
Single-label stock solution.
3.9 UV absorber mixed standard stock solution. accurately pipette 1 mL of the above 4 single standard stock solutions (3.8) to 10 mL volume
In the bottle (4.7), use methanol (3.1) to make a constant volume and prepare a UV absorber mixed standard stock solution with a concentration of 100 mg/L.
3.10 Mixed standard working solution. accurately pipette 0.05 mL, 0.1 mL, 0.2 mL, 0.5 mL, 1 mL, 2 mL, 5 mL of the above mixture
The standard stock solution (3.9) is placed in 7 10 mL volumetric flasks (4.7), and the volume is fixed with methanol (3.1), and the concentration is 0.5 mg/L, 1
Mixed standard working solutions of mg/L, 2 mg/L, 5 mg/L, 10 mg/L, 20 mg/L, 50 mg/L.
3.11 Silica gel cartridge (6 mL, 1 g). activate with 6 mL methanol (3.1) before use and keep it wet.
3.12 Microporous membrane. 0.2 μm pore size, organic type.
4 Instruments and equipment
4.1 Gas Chromatography Mass Spectrometer. Equipped with EI source.
4.2 Analytical balance. Sensitivity 0.1 mg.
4.3 Ultrasonic generator.
4.4 Rotary evaporator.
4.5 Pipette. 0 mL ~ 10 mL.
4.6 Conical flask with stopper. 50 mL.
4.7 Volumetric flask. 10 mL.
4.8 Round bottom flask. 50 mL.
4.9 Glass sheet. 10 cm×20 cm.
5 Sample preparation
Stir the sample evenly and level it on a clean glass sheet (4.9) to form a thin film of appropriate thickness. Dry naturally in a ventilated place, and wait
After it is completely dry, scrape it off with a razor blade, cut into pieces and mix well.
6 Handling of samples
6.1 Extraction
Accurately weigh 0.5 g of the air-dried sample (accurate to 0.1 mg), place it in a 50 mL conical flask (4.6) with a stopper, and add 20 mL of
Extraction agent, ultrasonic extraction for 20 min. Carefully transfer the supernatant into a 50 mL round-bottomed flask (4.8), rinse with 10 mL extractant 3 times
Put a stoppered Erlenmeyer flask (4.6), and put the eluent into a 50 mL round bottom flask (4.8). Concentrate to nearly 1 mL with a rotary evaporator (4.4),
To be purified.
Note. The extractant of solvent-based paint film is n-hexane (3.2), and the extractant of water-based paint film is acetonitrile (3.3).
6.2 Purification
Transfer the sample solution treated in 6.1 to the activated silica gel cartridge (3.11), and control the flow rate to 1 drop every 2 seconds. Use 6 mL
Elute with methanol (3.1), collect the eluate, and dilute to 10 mL with methanol (3.1). After being filtered by a microporous membrane (3.12), it is used for gas color
Spectrum-mass spectrometry.
6.3 Preparation of blank test solution
Except that no sample is added, all follow the above steps.
7 Determination
7.1 Gas chromatography-mass spectrometry conditions
Since the test results depend on the instrument used, it is impossible to give general parameters for gas chromatography/mass spectrometry. Set parameters
It should be ensured that the measured component and other components can be effectively separated during chromatographic determination. The following parameters are proved to be feasible.
a) Chromatographic column. DB-5 MS, 30 m × 0.25 mm (inner diameter) × 0.25 mm (film thickness), or equivalent performance.
b) Column temperature. 100 ℃ (1 min) 20 ℃/min.200 ℃ (1 min) 5 ℃/min 290 ℃ (5 min).
c) Temperature of the injection port. 280 ℃.
d) Chromatography-mass spectrometry interface temperature. 300 ℃.
e) Ion source temperature. 230 ℃.
f) Quadrupole temperature. 150 ℃.
g) Carrier gas. helium, purity ≥ 99.999%, 1.0 mL/min.
h) Ionization method. EI.
i) Ionization energy. 70 eV.
j) Mass scanning range. 50 amu ~ 450 amu.
k) Measurement method. SCAN mode.
l) Injection volume. 1.0 μL, without splitting.
m) Solvent delay. 4 min.
7.2 Drawing a standard working curve
According to the measurement conditions listed in 7.1, test the mixed standard working solution (3.10). Take the measured substance concentration as the abscissa, with
The peak area corresponding to the quantitative ion is the ordinate, and the standard working curve is drawn to obtain the linear equation. Typical gas phase of 4 kinds of UV absorbers
Refer to Appendix A for the total ion current diagram of Chromatography-Mass Spectrometer A.1.
7.3 Qualitative and quantitative analysis by gas chromatography-mass spectrometry
Analyze the liquid to be tested according to the above analysis conditions (7.1), according to the retention time of the chromatographic peak and the ultraviolet
The qualitative ion of the absorbent is qualitatively analyzed. Perform quantitative analysis according to the standard working curve (7.2).
7.4 Blank test
Carry out a blank test with the sample, and carry out pre-processing and testing according to the sample processing steps.
8 Calculation results
The content of various ultraviolet absorbers in the sample is calculated according to formula (1).
9 Lower limit of determination
The lower limit of the four ultraviolet absorbers in this method is 10 mg/kg.
10 Precision
The repeatability and reproducibility of the method are shown in Table 1 and Table 2.
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